CONTENT UNIFORMITY DETERMINATION OF IBUPROFEN INTACT TABLETS BY REFLECTANCE NIR SPECTROSCOPY

Ahmed Abouzaid

doi:10.21608/ajps.2017.28404

Abstract

Content uniformity (CU) is a critical quality attribute in tablet manufacturing process. The active pharmaceutical ingredient (API) is usually determined off-line techniques such as, high performance liquid chromatography (HPLC) which is a slow, destructive technique and requires sample preparation. Therefore, Near Infrared (NIR) spectroscopy was employed as a process analytical technology (PAT) tool to determine the API and consequently the content uniformity of tablets. NIR spectroscopy is a fast, non-destructive technique and requires minimal sample preparation. The purpose of this work was to develop and validate NIR reflectance method for the determination of the ibuprofen content (mg) for the content uniformity for ibuprofen tablet. Partial least squares (PLS) model for the NIR reflectance was constructed by using calibration laboratory tablets with different ibuprofen (IBU) contentsspanning from 146.47 mg to 243.91 mg. The predictive performance of the proposed method was evaluated by traditional chemometric criteria. The corresponding values for the root mean square error of prediction (RMSEP) were equal to 0.96% for NIR reflectance method. Besides, the proposed NIR method was successfully validated and implemented for the determination of the content uniformity for three batches that represent three levels of IBU content (160 mg, 200 mg and 240 mg).

Highlights

Content uniformity (CU) is a critical quality attribute in tablet manufacturing process(Djuris et al, 2013)
Samples are considered uniform if the drug content of each sample was within the limits established by both the European Pharmacopoeia (15% around the nominal content) and the US Pharmacopoeia (15% around the manufacturer’s label claim), and the relative standard deviation (RSD %) for the average of each batch was below the level required by the US Pharmacopoeia (6%) (Blanco et al, 2006)
The traditional chemometric criteria were calculated to evaluate the predictive ability of the developed Partial least squares (PLS) models(De Bleye et al, 2012).These criteria are regression coefficient (R2), the root mean squared error of cross-validation (RMSECV) and of prediction (RMSEP) for external validation set, not involved in the calibration set

Summary

Introduction

Content uniformity (CU) is a critical quality attribute in tablet manufacturing process(Djuris et al, 2013). Near Infrared (NIR) spectroscopy is currently used as a process analytical technology (PAT) tool to determine the API and the content uniformity of tablets (Blanco & Alcalá, 2006; Moes et al, 2008; Pestieau et al, 2014). NIR spectroscopy is a rapid, nondestructive and requires minimal sample preparation(Blanco et al, 2008) This technique has been applied for thedetermination of the chemical properties (e.g. active ingredient) and the physical properties (e.g. particle size) of the samples(Ciurczak et al, 1986; Frake et al, 1997). Vibrations of R–H, O–H, N–H, C–H and S–H bonds have strong overtones, as the dipole moment is high

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